CN108374160A - A kind of preparation method of high-quality titanium-based b-doped diamond film - Google Patents
A kind of preparation method of high-quality titanium-based b-doped diamond film Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/32—Carbides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
- C23C16/276—Diamond only using plasma jets
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/32—Carbides
- C23C16/325—Silicon carbide
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
- C23C16/513—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using plasma jets
Abstract
The present invention relates to a kind of preparation methods of high-quality titanium-based b-doped diamond film, including (1) Ar, C ion bombardment to form TiC on titanium surface, and titanium hydrogen alloy-layer is avoided to be formed；(2) transition zone SiC is deposited on TiC in favor of diamond nucleation；(3) the forming core stage constrains H ions with high-intensity magnetic field, and higher C/H ratios are obtained in workpiece surface.It is aided with Ar, C ion bombardment simultaneously, surface of SiC diamond phase is made preferentially to be formed；(4) depositional phase reduces magnetic field intensity, reduces constraint of the magnetic field to H ions, achievees the purpose that reduce workpiece surface C/H than being conducive to the growth of high-quality b-doped diamond film.Method provided by the invention avoids brittlement phase titanium hydrogen alloy-layer from being formed before boron-doped diamond forming core, by ion bombardment.With rich C ion bombardments in nucleation process, diamond phase is preferentially generated.The ratio of diamond phase in the binding force and film layer of these key links raising boron-doped diamond, to obtain high-quality b-doped diamond film in titanium-based workpiece surface.
Description
Technical field
The invention belongs to diamond coatings preparation fields, are related to a kind of new side depositing b-doped diamond film on titanium
Method.
Background technology
Earlier 2000s, with going deep into for b-doped diamond film research, the material is during degradation of organic waste water
Present efficiently, wide spectrum, longevity the features such as, field for the treatment of of water pollution have excellent application prospect.Currently, using in the world
B-doped diamond film is deposited by Hot Filament Chemical Vapor method in silicon substrate and niobium base.But the height of the property and niobium not easy to be processed of silicon
Heavy price lattice all become the obstacle of boron-doped diamond electrode material popularization and application.Newest research hotspot is to deposit to mix in titanium-based
Boron diamond electrode.However, metallic titanium surface hydrogen-absorbing ability is very strong, titanium hydrogen alloy-layer can be formed on surface layer, the brittlement phase is substantially
Degree reduces the binding force of b-doped diamond film and titanium-based material, while forming core to diamond and growing all adversely affects.
Therefore, deposition of high-quality boron-doped diamond becomes a difficult point in titanium-based.New studies have shown that ion bombardment is for diamond
Forming core have special role.Hot-wire chemical gas-phase deposition technology is to allow reaching of workpiece by the way of filament heating
Learn the condition of reaction.This method ionization level is low, even if applying back bias voltage on workpiece, can not still obtain ideal ion bombardment
Effect.The advantages of how ion bombardment being applied in the deposition of titanium-based b-doped diamond film, give full play to ion bombardment, keeps away
Exempt from its disadvantage, is the key that obtain high-quality titanium-based b-doped diamond film.
Invention content
To solve the above-mentioned problems, the present invention provides a kind of preparation method of high-quality titanium-based b-doped diamond film,
Its device being related to includes：Vacuum chamber, titanium-based workpiece, work rest, anode, plasma column, cathode, electromagnetic coil composition are mixed
Boron diamond deposition system, preparation process include：
(1) titanium-based workpiece is installed on work rest in a vacuum chamber, is evacuated to back end vacuum；
(2) it is passed through high-purity Ar, adjusts the vacuum degree that Ar flows reach setting, direct current is formed in cathode and positive interpolar discharge
Arc stretches plasma column, adjusts arc current to setting value；
(3) it is passed through H2And CH4, adjust H2Flow and CH4Flow reaches setting vacuum degree, is formed under action of plasma
Ar ions, C ions and H ions etc.；
(4) apply field supply to electromagnetic coil, form high-intensity magnetic field in vacuum chamber, height is formed in titanium-based workpiece surface
C/H ratios；
(5) apply back bias voltage on titanium-based workpiece so that Ar ions, the C ion bombardment titanium-based workpiece of plasma column outer layer
Surface forms TiC enriched layers, and continues setting time；
(6) back bias voltage is closed, the SiH of setting is passed through4Flow continues setting time, transition zone is formed on TiC enriched layers
SiC；
(7) SiH is closed4, it is passed through the B of setting2H6Flow adjusts the field supply in electromagnetic coil, while in titanium-based workpiece
Upper application back bias voltage so that Ar, C plasma constantly bombard titanium-based workpiece surface, preferential growth diamond phase, which persistently sets
It fixes time；
(8) back bias voltage is closed, reduces the field supply in electromagnetic coil to reduce the indoor magnetic field intensity of vacuum, adjusts
H2, CH4, B2H6Flow obtains the b-doped diamond film of expected thickness by controlling sedimentation time.
The preparation method of a kind of high-quality titanium-based b-doped diamond film, which is characterized in that described in step (1)
Back end vacuum is better than 1Pa.
The preparation method of a kind of high-quality titanium-based b-doped diamond film, which is characterized in that described in step (2)
Ar flows are 0.5~5SLM, and vacuum degree is 100~500Pa, and arc current is 80~200A.
The preparation method of a kind of high-quality titanium-based b-doped diamond film, which is characterized in that described in step (3)
H2Flow is 50~500sccm, CH4Flow is 5~100sccm, and vacuum degree is 500~1500Pa.
The preparation method of a kind of high-quality titanium-based b-doped diamond film, which is characterized in that described in step (4)
Field supply is 40~60A.
The preparation method of a kind of high-quality titanium-based b-doped diamond film, which is characterized in that described in step (5)
Back bias voltage is 50~250V, and setting time is 5~30min.
A kind of preparation method of high-quality titanium-based b-doped diamond film, which is characterized in that step (6) described step
Rapid SiH4Flow is 5~100sccm, and setting time is 5~30min.
The preparation method of a kind of high-quality titanium-based b-doped diamond film, which is characterized in that described in step (7)
B2H6Flow is 0.1~10sccm, and field supply is 40~60A, and back bias voltage is 100~250V, and setting time is 5~180min.
The preparation method of a kind of high-quality titanium-based b-doped diamond film, which is characterized in that described in step (8)
Field supply is 10~30A, H2Flow is 10~500sccm, CH4Flow is 1~100sccm, B2H6Flow be 0.1~
10sccm, 0.1~1000h of sedimentation time.
The technical scheme is that using the high feature of DC electric arc plasma chemical vapor deposition apparatus ionization level,
Generate a variety of charged ions.Advantageous Ar ions and C ion pair titanium-based materials is selected to carry out the bombardment of appropriate energy using high-intensity magnetic field,
Ti-H keys (bond energy 226.6kJ/mol) are interrupted, and Ti-C keys (bond energy 423kJ/mol) are retained, and titanium-based surface is progressively enriched with Ti-
C keys form TiC enriched layers on surface, while bombardment avoids the formation of titanium hydrogen brittleness phase layer；Deposition of SiC layer on it again；It utilizes
High-intensity magnetic field constrains H ions, and titanium substrate surface is made to form high C/H ratios, improves Enhancing Nucleation Density；Using Ar ions and C ion bombardments,
Improve the ratio of diamond phase in the minds of diamond nuclei；Magnetic field intensity is finally reduced, so that the C/H ratios of titanium substrate surface is reduced, to obtain
Obtain the b-doped diamond film of high-quality.
Description of the drawings
Attached drawing is the schematic device for being used to prepare high-quality titanium-based b-doped diamond film.
Specific implementation mode
The invention will be further described below：
Embodiment 1：
50 millimeters of outer diameter, 2 milli of wall thickness are installed on the work rest 3 of DC electric arc plasma chemical vapor deposition apparatus
Rice, long 300 millimeters of titanium tube 2,2 70 millimeters of centre-to-centre spacing vacuum chamber center of titanium tube.Specific operation process is as follows：It 1) will with vacuum pump
The back end vacuum of vacuum chamber 1 is evacuated to 1Pa or less.2) it is passed through the Ar that flow is 1.5SLM, control vacuum degree in vacuum chamber is 300Pa.
Electric discharge generates plasma column 5 between cathode 4 and anode 6, and adjusting arc current is 100A.3) it is 200sccm's to be passed through flow
H2With the CH that flow is 40sccm4, vacuum degree is adjusted to 1200Pa.4) field supply of magnetic coil 7 is adjusted to 50A.5) titanium is rotated
Pipe 2, and in titanium tube 2 apply 100V back bias voltage, continue 20 minutes, prepare TiC enriched layers.6) it is 30sccm's to be passed through flow
SiH4, adjust titanium tube negative bias and be depressed into 0V, continue 10 minutes, deposit SiC transition zones.7) SiH is closed4, it is 5sccm's to be passed through flow
B2H6.Maintain 7 field supply 50A of magnetic coil.It adjusts 2 negative bias of titanium tube and is depressed into 150V.The nucleation process for carrying out boron-doped diamond, holds
The continuous 60 minutes time.8) 7 field supply of magnetic coil is decreased to 15A.Adjust H2Flow is 150sccm, CH4Flow is 20sccm,
B2H6Flow is 2.5sccm, carries out the deposition of 20 hours b-doped diamond films.
The vacuum environment better than 1Pa is obtained in the present embodiment first.Then Ar ions are selected under the conditions of 50A field supplies
With C ions with the energy bombardment titanium tube surface of 100V back bias voltages, Ti-H keys are interrupted, Ti-C keys are retained, TiC enriched layers is obtained, keeps away
Exempt from the formation of titanium hydrogen brittleness phase layer.Then in 20 minutes SiC layers of titanium-based material superficial deposit as diamond nucleation substrate；Apply again
The field supply of 50A improves the C/H ratios on titanium tube surface, to improve the Enhancing Nucleation Density of diamond；Meanwhile applying in titanium tube
The back bias voltage of 150V utilizes the Ar ions and C ion bombardments of appropriate energy, removal C sp2Key retains C sp3Key improves Buddha's warrior attendant
The ratio of diamond phase in the minds of lithophysa；Field supply is finally reduced to 15A, so that the C/H ratios of titanium substrate surface is reduced, to obtain height
The b-doped diamond film of quality.
Claims (9)
1. a kind of preparation method of novel high-quality titanium-based b-doped diamond film, the device being related to include：Vacuum chamber (1),
Titanium-based workpiece (2), work rest (3), anode (4), plasma column (5), cathode (6), the boron-doping Buddha's warrior attendant of electromagnetic coil (7) composition
Stone depositing system, preparation process include：
(1) titanium-based workpiece (2) is mounted on the work rest (3) in vacuum chamber (1), is evacuated to back end vacuum；
(2) it is passed through high-purity Ar, adjusts the vacuum degree that Ar flows reach setting, discharging between cathode (6) and anode (4) forms direct current
Electric arc stretches plasma column (5), adjusts arc current to setting value；
(3) it is passed through H2And CH4, adjust H2Flow and CH4Flow reaches setting vacuum degree, under action of plasma formed Ar from
Son, C ions and H ions etc.；
(4) it gives electromagnetic coil (7) to apply field supply, forms high-intensity magnetic field in vacuum chamber, formed on titanium-based workpiece (2) surface
High C/H ratios；
(5) apply back bias voltage on titanium-based workpiece (2) so that the Ar ions of plasma column (5) outer layer, C ion bombardment titanium-based works
Part (2) surface forms TiC enriched layers, and continues setting time；
(6) back bias voltage is closed, the SiH of setting is passed through4Flow continues setting time, and transition zone SiC is formed on TiC enriched layers；
(7) SiH is closed4, it is passed through the B of setting2H6Flow adjusts the field supply in electromagnetic coil (7), while in titanium-based workpiece
(2) apply back bias voltage on so that Ar, C plasma constantly bombard titanium-based workpiece (2) surface, preferential growth diamond phase, the stage
Continue setting time；
(8) back bias voltage is closed, reduces the field supply in electromagnetic coil (7) to reduce the magnetic field intensity in vacuum chamber (1), adjusts
H2, CH4, B2H6Flow obtains the b-doped diamond film of expected thickness by controlling sedimentation time.
2. a kind of preparation method of novel high-quality titanium-based b-doped diamond film according to claim 1, feature exist
In the back end vacuum described in step (1) is better than 1Pa.
3. a kind of preparation method of novel high-quality titanium-based b-doped diamond film according to claim 1, feature exist
In the Ar flows described in step (2) are 0.5~5SLM, and vacuum degree is 100~500Pa, and arc current is 80~200A.
4. a kind of preparation method of novel high-quality titanium-based b-doped diamond film according to claim 1, feature exist
In the H described in step (3)2Flow is 50~500sccm, CH4Flow is 5~100sccm, and vacuum degree is 500~1500Pa.
5. a kind of preparation method of novel high-quality titanium-based b-doped diamond film according to claim 1, feature exist
In the field supply described in step (4) is 40~60A.
6. a kind of preparation method of novel high-quality titanium-based b-doped diamond film according to claim 1, feature exist
In the back bias voltage described in step (5) is 50~250V, and setting time is 5~30min.
7. a kind of preparation method of novel high-quality titanium-based b-doped diamond film according to claim 1, feature exist
In step (6) the step SiH4Flow is 5~100sccm, and setting time is 5~30min.
8. a kind of preparation method of novel high-quality titanium-based b-doped diamond film according to claim 1, feature exist
In the B described in step (7)2H6Flow is 0.1~10sccm, and field supply is 40~60A, and back bias voltage is 100~250V, setting
Time is 5~180min.
9. a kind of preparation method of novel high-quality titanium-based b-doped diamond film according to claim 1, feature exist
In the field supply described in step (8) is 10~30A, H2Flow is 10~500sccm, CH4Flow is 1~100sccm, B2H6
Flow is 0.1~10sccm, 0.1~1000h of sedimentation time.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112030133A (en) * | 2020-11-06 | 2020-12-04 | 苏州香榭轩表面工程技术咨询有限公司 | Diamond and preparation method and application thereof |
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| US20040137147A1 (en) * | 2000-12-29 | 2004-07-15 | O'donnell Robert J. | Boron nitride/yttria composite components of semiconductor processing equipment and method of manufacturing thereof |
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| JP2014118627A (en) * | 2012-12-19 | 2014-06-30 | Taiyo Kagaku Kogyo Kk | Thin film formed on intermediate layer comprising nonmagnetic material |
| CN105887038A (en) * | 2016-04-15 | 2016-08-24 | 天津理工大学 | Method for etching boron-doped diamonds |
| CN106435518A (en) * | 2016-10-21 | 2017-02-22 | 中南大学 | High-specific-surface-area boron-doped diamond electrode and preparation method and application thereof |
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| US5645900A (en) * | 1993-04-22 | 1997-07-08 | The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration | Diamond composite films for protective coatings on metals and method of formation |
| US20040137147A1 (en) * | 2000-12-29 | 2004-07-15 | O'donnell Robert J. | Boron nitride/yttria composite components of semiconductor processing equipment and method of manufacturing thereof |
| JP2014118627A (en) * | 2012-12-19 | 2014-06-30 | Taiyo Kagaku Kogyo Kk | Thin film formed on intermediate layer comprising nonmagnetic material |
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| CN103695863A (en) * | 2013-12-09 | 2014-04-02 | 四川大学 | Preparation method of boron-doped diamond film/carbon film composite electrode material |
| CN105887038A (en) * | 2016-04-15 | 2016-08-24 | 天津理工大学 | Method for etching boron-doped diamonds |
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